Synthesis Methodology to Produce Nano Metal Organic Framework Crystals

Abstract

A method for synthesizing particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm. A base compound is added to a solution of a metal salt and an organic polydentate ligand with thorough stirring at a temperature between about 15° C. and about 30° C. for a time less than about 4 hours.

1 . A method for synthesizing particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm, said method comprising rapidly stirring at a temperature between about 15° C. and about 30° C. and for a time less than about 4 hours a solution comprising a metal salt and an organic polydentate ligand in solvent while adding a base compound capable of deprotonating the ligand to form a nano-metal organic framework crystals, wherein the ratio of base compound to acid function within the ligand in the solution is less than about 2:1. 
     
     
         2 . The method of  claim 1  wherein ligand is selected from the group consisting of neutral bidentate ligands, 1,4-benzene dicarboxylic acid, 1,3,5-benzene tricarboxylic acid, 1,2,4,5-benzene tetracarboxylic acid, and blends thereof. 
     
     
         3 . The method of  claim 1  wherein the ratio of base compound to acid function is between about 0.25:1 and 1.75:1. 
     
     
         4 . The method of  claim 1 , wherein the solution further comprises additive selected from the group consisting of Brij surfactants, straight chain paraffins concatenated with plural ether moieties and capped with a hydroxyl moiety, and blends thereof. 
     
     
         5 . The method of  claim 1 , wherein the total molal concentration of concentration of metal salt and ligand is between about 0.03 M and about 0.15 M. 
     
     
         6 . A particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm made in accordance with the method of  claim 1 . 
     
     
         7 . The nano-metal organic framework crystals of  claim 6  having a specific surface area comprising greater than about 50 percent mesoporosity. 
     
     
         8 . A method for synthesizing particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm, said method comprising rapidly stirring at a temperature between about 15° C. and about 30° C. and for a time less than about 4 hours a solution comprising a metal salt and an organic polydentate ligand in solvent while adding a base compound capable of deprotonating the ligand to form a nano-metal organic framework crystals, wherein the total molal concentration of metal and ligand in the solvent is at least about 0.08 M. 
     
     
         9 . The method of  claim 8  wherein ligand is selected from the group consisting of neutral bidentate ligands, 1,4-benzene dicarboxylic acid, 1,3,5-benzene tricarboxylic acid, 1,2,4,5-benzene tetracarboxylic acid, and blends thereof. 
     
     
         10 . The method of  claim 8  wherein the ratio of base compound to acid function is between about 0.25:1 and 1.75:1. 
     
     
         11 . The method of  claim 8 , wherein the solution further comprises an additive. 
     
     
         12 . The method of  claim 11 , wherein the additive is selected from the group consisting of Brij surfactants, straight chain paraffins concatenated with plural ether moieties and capped with a hydroxyl moiety, and blends thereof. 
     
     
         13 . A particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm made in accordance with the method of  claim 8 . 
     
     
         14 . The nano-metal organic framework crystals of  claim 13  having a specific surface area comprising greater than about 50 percent mesoporosity. 
     
     
         15 . A method for synthesizing particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm, said method comprising rapidly stirring at a temperature between about 15° C. and about 30° C. and for a time less than about 4 hours a solution comprising a metal salt and an organic polydentate ligand in solvent while adding a base compound capable of deprotonating the ligand to form a nano-metal organic framework crystals, wherein the solvent comprises at least two solvents. 
     
     
         16 . The method of  claim 15  wherein the ratio of base compound to acid function is between about 0.25:1 and 1.75:1. 
     
     
         17 . The method of  claim 15 , wherein the solution further comprises additive selected from the group consisting of Brij surfactants, straight chain paraffins concatenated with plural ether moieties and capped with a hydroxyl moiety, and blends thereof. 
     
     
         18 . The method of  claim 15 , wherein the total molal concentration of concentration of metal salt and ligand is between about 0.03 M and about 0.15 M. 
     
     
         19 . Particulate or loosely agglomerated nano-metal organic framework crystals having an average particle size less than 100 nm made in accordance with the method of  claim 15 . 
     
     
         20 . The nano-metal organic framework crystals of  claim 19  having a specific surface area comprising greater than about 50 percent mesoporosity.